HRID1441145

反应详情

EQUATION

反应方程式

HRID 1441145 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 5 liter three neck round bottom flask, equipped with a mechanical stirrer and reflux condenser, was charged with 300 g (1.16 moles) of 99% hexadecanolide, 1000 mls of 50% sodium hydroxide, 1500 mls of toluene and 5.6 g (0.01 6 moles) of 97% tetrabutylammonium hydrogen sulfate. The reaction mixture stirred at 85°-95° C. overnight, the reaction was cooled, and filtered under vacuum. The filtered solid was washed with diethyl ether before being added to water and acidified to pH=1.5 with concentrated hydrochloric acid. The precipitated product was filtered under vacuum, washed several times with water and dried at 50°-60° C. under high vacuum to give 353 g (1.2 moles) of 97% 16-hydroxy hexadecanoic acid.

WORKUP

后处理

  1. temperaturereflux condenser
  2. temperaturethe reaction was cooled
  3. filtrationfiltered under vacuum
  4. washThe filtered solid was washed with diethyl ether
  5. additionbefore being added to water
  6. filtrationThe precipitated product was filtered under vacuum
  7. washwashed several times with water
  8. customdried at 50°-60° C. under high vacuum